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Original Article
sequentially may lead to the slightly increased in the energy gap. Also found that it is in the range of semiconductor
materials.
KEYWORDS: Sol-Gel Autocombustion Method, Ferrite Nanoparticles, Optical Properties and XRD
Received: Dec 06, 2016; Accepted: Jan 05, 2017; Published: Jan 12, 2017; Paper Id.: IJNAFEB20171
INTRODUCTION
Nanotechnology is the combination of the branches of science such as engineering, physics, chemical
engineering, medical biology and the applications of nanomaterials1; which are applicable in electromechanical
devices, optical devices, magnetic devices, and tissue engineering2. The attractive, qualitative, intelligent
functional materials, components and systems are designed by new material nanotechnology technique3-4. Superior
physical properties of ferrites like recording are used for magnetic resonance imaging enhancement, catalysis, and
sensors5. The MFe2O4 is the chemical formula of spinel ferrites where M is divalent metal cations6. Magnesium
ferrite (MgFe2O4) has an inverse spinel structure in which Mg2+ cations are on octahedral sites and zinc ferrite
(ZnFe2O4) has normal spinel structure in which Zn2+ cations occupy tetrahedral sites7-10. The intensive properties
of the small scale size spinel ferrites were used for biomedical applications11-13. The co-precipitation,
hydrothermal, sol-gel, etc techniques were used to produce high quality nanoparticle and particle size in the range
between 2 to 100 nm14-15.
In this work, Ni0.4 Mg0.4 Cd0.2 Yy Fe2-y O4 Nanoferrites (where y = 0.025 to 0.125) were synthesized using
co-precipitation methods. X-ray diffraction (XRD) was used in order to investigate the structural of Y3+ substituted
nickel-magnesium-cadmium nano-ferrites and to determine the lattice parameters and the space group symmetry.
Ultraviolet visible spectrometer (UV-Vis) and Fourier Transform Infrared Spectroscopy (FTIR) were used to
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2 R.B. Bhise & S.M. Rathod
The Y3+ doped in Ni-Mg-Cd ferrite powders were synthesized by sol-gel autocombustion method at low
temperatures for different compositions of Ni0.4 Mg0.4 Cd0.2 Yy Fe2-y O4 (where y = 0.025, 0.050, 0.075, 0.100 and 0.125).
According to respective molar amounts of yttrium nitrate, magnesium nitrate, nickel nitrate, cadmium nitrate, ferric nitrate
of AR grade with 99% purity and citric acid as a fuel were used with stoichiometric ratio (1:3) proportion to obtain the
final product16. All these chemicals were dissolved in double distilled water and stirred till to obtain the homogeneous
solution. Ammonium hydroxide was added drop by drop to maintain pH between 7 to 8 during the stirring process and
solution was continuously stirred with 80-100 C for about 4-5 hours to obtain sol. After 4-5 hours, gel converts into ash
and ash convert into powder. Finally get fine powder of Ni0.4 Mg0.4 Cd0.2 Yy Fe2-y O4 ferrite nanoparticles after auto
combustion. The powder was sintered at 400 C for 2 hours.
The X-ray diffractometer (Cu-K radiation of wavelength 1.54 A0 at 40 kV) were performed a scanning 20 to 80
degree with step of 0.02 degree per second for each prepared sample to study structural characterization and used to
determine lattice parameter with grain size. The optical characteristics was studied using Fourier Transformation Infrared
spectroscopy (FT-IR) of Bruker 3000 Hyperion microscope with vertex 80 single point detector performing images
resolution ranging between 7500 to 450 cm-1 and UV-Visible spectroscopy. Further investigations of the optical properties
are under way to elucidate the effective role of inter particle interactions in these samples.
XRD Analysis: The prepared powders of Y3+ doped Ni-Mg-Cd nanoferrite were characterized by X-ray
diffraction and pattern of sintered powder is shown in figure-1. The XRD pattern conform the formation of a homogeneous
spinal cubic structure and the broad peaks indicates fine particle nature of the nanoparticles. Scherers formula was used to
determine the particle (grain) size.
.
t= (1)
The average particle (grain) size of nanoparticles was noted in table-1 and it is ranging between 17 to 25 nm. This
indicates if the concentration of Y3+ doped increases then average particle size decreases. Lattice parameters were
calculated for sintered sample is ranging from 1.9228 to 2.1300 A0. The value of lattice constant of Ni-Mg-Cd ferrite
shows the expansion of unit cell with rare earth yttrium doping when compared with pure yttrium ferrite and the deviation
in lattice parameter attributed to the cations rearrangement in the nanosize prepared ferrites. The Y3+ substituted ferrites
have high stability relative to Ni-Mg-Cd ferrite due to doping of large ionic radius of Y3+ ions (0.9 A0) with small ionic
radius Fe3+ ions (0.645 A0).
Table 1: The Grain Size of Prepared Samples Ni0.4 Mg0.4 Cd0.2 Yy Fe2-y O4 by x-Ray Diffraction
Obs. No. Composition Grain size (t) nm Lattice constant (a) Ao
1 y = 0.025 23 2.1309
2 y = 0.050 25 2.1338
3 y = 0.075 21 2.1305
4 y = 0.100 22 2.1300
5 y = 0.125 17 1.9228
Optical Studies
FTIR Analysis: In order to investigate the chemical functional groups on the synthesized Ni0.4 Mg0.4 Cd0.2 Yy Fe2-y
O4, FTIR spectroscopy are performed. The FTIR spectra of the prepared Ni0.4 Mg0.4 Cd0.2 Y0.100 Fe1.900 O4 are shown in
figure 2 to know the bonding characteristics of the materials. The peaks at 429.68 cm-1 and 554.13 cm-1 are the peaks of
Fe-O bond in Y doped Ni-Mg-Cd ferrite and it is arises due to the lattice vibrations of the oxide ions against cations.
The peak at 1384.13 cm-1 indicates the presence of O-H bond due to bending vibration. The broad peak at 3434.50 cm-1
gives presence of hydroxyl group in the material and indicates that the material absorbed moisture from atmosphere during
analysis.
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4 R.B. Bhise & S.M. Rathod
The intense absorption bond is observed at 554.13 cm-1 which shows the characteristic bond of spinel structure
which may due to presence of Fe-O and Y-O bonds or crystalline nature of Y doped Ni-Mg-Cd ferrite. Hence, FT-IR
analysis supports the observation of XRD analysis and confirms the crystalline nature of ferrite. So, the peaks at 476 cm-1
and 1058 cm-1 confirms the presence of yttrium doped in Ni-Mg-Cd ferrite. Finally, the doping of Y3+ on Ni-Mg-Cd ferrite
was confirmed by different pattern of the plots and the difference in relative position and intensity of the peaks appeared in
the FT-IR plots of the prepared samples. This indicates normal ferromagnetic materials.
UV-Visible Analysis: The figure-3 shows optical properties were studied from UV-Visible spectroscopy to
calculate the band gap energy. In the absorption molecules of non-bonding electrons can absorb the energy in the form of
ultraviolet or visible light to excite this electron to higher or anti-bonding molecular orbit. The energy band gap was
calculated for samples with different ratio using following formula;
E= (2)
Energy band gap was found to be 3.9935, 4.0390, 4.0655, 4.1196 and 4.1541 eV. The substitution was resulted in
slight increase in the lattice constant and that sequentially may lead to the slightly decrease in the energy gap. The average
Band gap of prepared sample is 4.0743 eV and wavelength absorb by 508 nm. It is in the range of semiconductor materials.
Table 2: The Band Gap Energy of Ni0.4 Mg0.4 Cd0.2 Yy Fe2-y O4 by UV-Visible Spectroscopy
Obs. No. Composition Wavelength (nm) Band gap energy (eV)
1 y=0.025 310.5 3.9935
2 y=0.050 307.0 4.0390
3 y=0.075 305.0 4.0655
4 y=0.100 301.0 4.1196
5 y=0.125 298.5 4.1541
CONCLUSIONS
The Ni0.4 Mg0.4 Cd0.2 Yy Fe2-y O4 nanoferrites were synthesized using sol-gel autocombustion technique. The
increase in the Y3+ concentration gives the significant changes in the particle size and optical properties of the composition
Ni0.4 Mg0.4 Cd0.2 Yy Fe2-y O4 (where y = 0.025, 0.050, 0.075, 0.100 and 0.125). The FT-IR spectroscopy study shows two
main metal oxygen bands in the range of 429.68 to 554.13 cm-1 confirms the formation of cubic spinel phase structure of
Y3+ substitute in Ni-Mg-Cd ferrite. The synthesis of nanoparticles with crystalline size decreases and lattice constant
increases as the concentration increases and is in the range of 17 to 25 nm for 400 oC. The UV-Visible analysis shows band
gap energy increases with increase in Y3+ concentration. The UV-Visible study shows average Band gap energy is 4.0743
eV and wavelength absorb by 508 nm. This result prepared ferrite materials is in the range of semiconductor materials.
ACKNOWLEDGEMENTS
The authors are thankful to IIT, Powai (Mumbai), Savitribai Phule Pune University, Abasaheb Garware,
College, Pune and PDEs Baburaoji Gholap College, New Sangavi, Pune, India for providing the instrumental
facilities for the characterization purpose.
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